CN102641387A - Method for supercritically extracting natural activity ingredient oil tea polyphenol from oil tea fruits - Google Patents

Abstract

The invention discloses a method for supercritically extracting natural activity ingredient oil tea polyphenol from oil tea fruits, which belongs to the technical field of oil tea polyphenol extraction. The method comprises the following steps: oil tea fruits are used as raw materials to be dried and smashed; supercritical CO2 is used for removing tea oil from oil tea seeds, oil-removed oil tea seeds are mixed with hulls or used independently, oil tea fruit hulls are used as raw materials to supercritically extract oil tea polyphenol, and an entrainer is injected in dynamic entrainment mode to perform supercritical CO2 extraction to achieve oil tea polyphenol. Compared with a traditional solvent formulation method, the method is high in utilization rate of resources, low in toxicity of the entrainer in the whole process, small in using amount, simple in process and environment-friendly.

Description

Method from oil tea fruit supercritical extraction active skull cap components oil tea polyphenol

Technical field

The present invention relates to a kind of method, belong to the oil tea polyphenol and extract the skill technical field from oil tea fruit supercritical extraction active skull cap components oil tea polyphenol.

Background technology

Oil tea is the distinctive a kind of woody edible oil materials seeds of China, with olive oil, Cortex cocois radicis, Elaeis guineensis Jacq. and be called the world four big woody oleiferous plants plants.Mainly concentrate on the oil tea saponin aspect for extraction of active ingredients in the oil tea at present, but go deep into along with what study, many functions of oil tea polyphenols come to light.Tea polyphenols is owing to the substituted high response of its hydroxyl and engulf the ability of free radical, and has good non-oxidizability.Discover; The oil tea polyphenol not only has good non-oxidizability; And can also delay the aging of body; Suppress the generation of diseases such as cancer, diabetes, cataract, atherosclerosis, renal glomerular disease, myocardial infarction, so the tea polyphenols product is mainly used in fields such as medicine, food antiseptic.

The method of Extraction oil tea polyphenols mainly contains solvent method, the sedimentation method and absorption method at present.Though solvent method technology is simple, is suitable for large-scale production, the production cycle is long, temperature is high, tea polyphenols is prone to the oxidation inactivation; In the process of producing, use a large amount of organic solvents simultaneously; Operate safety inadequately, environment is polluted, do not meet the developing direction of " Green Chemistry "; The sedimentation method mainly utilize metal ion and polyphenol to form complex, from solution, are precipitated out, and the back makes polyphenol from deposition, dissociate out with the acid dissolving, and this method organic solvent amount is bigger, and mixes metal ion; Absorption method mainly is through behind the organic solvent extraction, utilizes the resin absorption separating tea multi-phenol, and this method later separation is more loaded down with trivial details.Supercritical extraction technique not only can guarantee product quality and biological activity thereof to greatest extent as a kind of novel separation method, and productive rate is high, and experimental repeatability is strong, and later separation is simple.It is raw material that patent CN101194713, CN102041164A relate separately to the Semen Camelliae, adopt supercritical extraction technique or ultrasonic auxiliary subcritical abstraction technology to extract the method for Oleum Camelliae, but all oil tea is not further developed.

Summary of the invention

The object of the present invention is to provide a kind of method from oil tea fruit supercritical extraction active skull cap components oil tea polyphenol, this method not only extraction ratio is high, and product purity is high, and product is easy to separate.

The present invention realizes through following technical scheme.A kind of method from oil tea fruit supercritical extraction active skull cap components oil tea polyphenol is characterized in that comprising following process:

(1) oil tea Semen Camelliae and the shell that obtains that really shell carried out drying respectively, make its moisture mass content be lower than 4%;

(2) with dried Semen Camelliae and shell pulverize separately to 20 orders, subsequent use;

(3) extraction of Oleum Camelliae: the Semen Camelliae powder of step (2) gained is added extraction kettle; At pressure is 15-45 MPa, and the flow velocity with CO under temperature 35-65 ℃ is that 30-150 L/h removes Oleum Camelliae 1.5-4h, and the CO that comes out from extraction kettle gets into knockout drum; Temperature be 35-65 ℃ with pressure 10-20 MPa under carry out flash trapping stage; Then temperature 20-40 ℃ with pressure 4-7 MPa under carry out secondary and separate, in knockout drum, obtain Oleum Camelliae, the CO that separates ₂Recycle after filtration and refrigeration system pressurization again;

(4) will pass through the shell that step (3) takes off the pulverizing that Semen Camelliae or step (2) behind the Oleum Camelliae obtain adds in the extraction kettle respectively; Or the shell of the pulverizing that will obtain through the Semen Camelliae after Oleum Camelliae is taken off in step (3) and step (2) adds in the extraction kettle together; Speed with 0.02-0.20 L/h in extraction kettle adds mass concentration 50-80% ethanol water entrainer; Or the adding mass concentration is a 50%-80% methanol aqueous solution entrainer; Or add the acetone entrainer or add the ethyl acetate entrainer, be to carry out supercritical CO extraction 0.5h-2.5 h under the 10-40 MPa at temperature 35-60 ℃ with pressure, in knockout drum, be 20-40 ℃ then with the temperature; Pressure is to isolate CO under the 4-7 MPa, obtains the solution of oil-containing tea polyphenols;

(5) step (4) gained oil-containing tea polyphenols solution decompression is steamed entrainer, obtain pale yellow powder shape solid.

The invention has the advantages that: at first the present invention takes supercritical to remove the Oleum Camelliae in the Semen Camelliae, advances one then

Go on foot the Extraction oil tea polyphenols, therefore improved the extraction ratio of oil tea polyphenol, in addition; In the process also with shell as one of raw material Extraction oil tea polyphenols, thereby improved the utilization rate of resource, the entrainer low toxicity that whole technology adopted; Use amount is few, and process is simple, environmental protection.

The specific embodiment

Instance 1:

With the oil tea separation of really shelling, take by weighing Semen Camelliae 300g, put into the dry 1h of baking oven, after the cooling Semen Camelliae 293.8g; Semen Camelliae after the oven dry is crushed to 50 orders, adds extraction kettle, the supercritical CO extraction conditions is: 45 ℃ of temperature; Pressure 30 MPa, CO flow velocity are 120 L/h, extraction 2h; In knockout drum, collect the light yellow transparence Oleum Camelliae of supercritical extraction gained, its quality is 88.9 g, and the Oleum Camelliae extraction rate is 29.63%.

Regulate the supercritical extraction condition, pressure is 20 MPa, and is temperature-resistant, in extraction kettle, adds the ethanol water of mass concentration 70% with the speed of 0.03 L/h, extracts 1.5 h, in knockout drum, collects extract.Adopt the method for rotary evaporation, under 55 ℃, remove the entrainer in the extract, obtain light yellow oil tea polyphenols pulverulent solids.Its quality is 15.51 g, and productive rate is 5.17%, and according to GB/T8313-2008, adopting the ultraviolet spectrophotometer analysis can get oil tea polyphenol purity is 86%.

Instance 2:

With the oil tea separation of really shelling, take by weighing Semen Camelliae 500 g, put into dry 3 h of baking oven, after the cooling Semen Camelliae 487.5g; And the Semen Camelliae after will drying is crushed to 40 orders, adds extraction kettle, and the condition of supercritical CO extraction is: 55 ℃ of temperature; Pressure 30 MPa, CO flow velocity are 120 L/h, extraction 3h; In knockout drum, collect the light yellow Oleum Camelliae of supercritical extraction gained, its quality is 141.8 g, and the Oleum Camelliae extraction rate is 28.35%.

Regulate the supercritical extraction condition, pressure is 25 MPa, and is temperature-resistant, injects the ethyl acetate entrainer with the speed of 0.07 L/h to extraction kettle, and the extraction time is 2 h, collects extract.Adopt the method for rotary evaporation, under 60 ℃, remove the entrainer in the extract, obtain light yellow oil tea polyphenols pulverulent solids.Its quality is 31.55 g, and productive rate is 6.31%, and according to GB/T8313-2008, adopting the ultraviolet spectrophotometer analysis can get oil tea polyphenol purity is 81%

Instance 3:

With the oil tea separation of really shelling, take by weighing Semen Camelliae 800 g, put into dry 3 h of baking oven; Get Semen Camelliae 777.5g after the cooling, the Semen Camelliae after the oven dry is crushed to 60 orders, drop into extraction kettle; The supercritical CO extraction conditions is: 45 ℃ of temperature, and pressure 35 MPa, CO flow velocity are 150 L/h extraction time 4h; In knockout drum, collect the light yellow transparence Oleum Camelliae of supercritical extraction gained, its quality is 249.4g, and the Oleum Camelliae extraction rate is 31.17%.

Regulate the supercritical extraction condition, pressure is 25 MPa, and is temperature-resistant, adds 60% ethanol water with the speed of 0.16L/h to extraction kettle, and the extraction time is 1 h, collects extract.Adopt the method for rotary evaporation, under 55 ℃, remove the entrainer in the extract, obtain light yellow oil tea polyphenols pulverulent solids.Its quality is 45.52 g, and productive rate is 5.69%, and according to GB/T8313-2008, adopting the ultraviolet spectrophotometer analysis can get oil tea polyphenol purity is 82%.

Instance 4:

Take by weighing oil-tea camellia husks 500g, put into the dry 3h of baking oven, obtain oil-tea camellia husks 495g; Oil-tea camellia husks after the oven dry is crushed to 50 orders, drops in the extraction kettle, temperature and pressure is set at 55 ℃ and 30MPa respectively; After waiting to stablize; Speed with 0.12L/h is injected acetone in extraction kettle, the extraction time is 1.5h, collects extract.Adopt the method for rotary evaporation, under 60 ℃, remove the entrainer in the extract, obtain light yellow oil tea polyphenols pulverulent solids; Its quality is 12.65g; Productive rate is 2.53%, and according to GB/T8313-2008, adopting the ultraviolet spectrophotometer analysis can get oil tea polyphenol purity is 82%.

Instance 5:

Take by weighing oil-tea camellia husks 300g, put into the dry 3h of baking oven, obtain oil-tea camellia husks 294g; Oil-tea camellia husks after the oven dry is crushed to 40 orders, drops in the extraction kettle, temperature and pressure is set at 45 ℃ and 25MPa respectively; After waiting to stablize; In extraction kettle, adding mass concentration with the speed of 0.09L/h is 70% ethanol water, and the extraction time is 2h, in knockout drum, collects extract.Adopt the method for rotary evaporation, under 55 ℃, remove the entrainer in the extract, obtain light yellow oil tea polyphenols pulverulent solids; Its quality is 9.36g; Productive rate is 3.12%, and according to GB/T8313-2008, adopting the ultraviolet spectrophotometer analysis can get oil tea polyphenol purity is 79%.

Instance 6:

With the oil tea separation of really shelling, put into dry 3 h of baking oven, Semen Camelliae after the oven dry and shell are pulverized; Take by weighing dried Semen Camelliae 300 g, drop into extraction kettle, the supercritical CO extraction conditions is: 35 ℃ of temperature; Pressure 25 MPa, CO flow velocity are 150 L/h, extraction time 1.5h; In knockout drum, collect the light yellow transparence Oleum Camelliae of supercritical extraction gained, its quality is 85.86g, and the Oleum Camelliae extraction rate is 28.62%.

Shell 100g in the Semen Camelliae that extracted Oleum Camelliae after the adding drying and crushing adds in the extraction kettle, at 45 ℃; Pressure is that to add mass concentration with the speed of 0.09L/h under the 30MPa be that 70% ethanol water carries out supercritical extraction 1.5h; Adopt the method for rotary evaporation, under 55 ℃, remove the entrainer in the extract, obtain yellow powder powder solid; Its quality is 17.96g; Productive rate is 4.49%, and according to GB/T8313-2008, adopting the ultraviolet spectrophotometer analysis can get oil tea polyphenol purity is 81%.

Claims (1)

1. method from oil tea fruit supercritical extraction active skull cap components oil tea polyphenol is characterized in that comprising following process:

(1) oil tea Semen Camelliae and the shell that obtains that really shell carried out drying respectively, make its moisture mass content be lower than 4%;

(2) with dried Semen Camelliae and shell pulverize separately to 20 orders, subsequent use;

(3) extraction of Oleum Camelliae: the Semen Camelliae powder of step (2) gained is added extraction kettle; At pressure is 15-45 MPa, and the flow velocity with CO under temperature 35-65 ℃ is that 30-150 L/h removes Oleum Camelliae 1.5-4h, and the CO that comes out from extraction kettle gets into knockout drum; Temperature be 35-65 ℃ with pressure 10-20 MPa under carry out flash trapping stage; Then temperature 20-40 ℃ with pressure 4-7 MPa under carry out secondary and separate, in knockout drum, obtain Oleum Camelliae, the CO that separates ₂Recycle after filtration and refrigeration system pressurization again;

(4) will pass through the shell that step (3) takes off the pulverizing that Semen Camelliae or step (2) behind the Oleum Camelliae obtain adds in the extraction kettle respectively; Or the shell of the pulverizing that will obtain through the Semen Camelliae after Oleum Camelliae is taken off in step (3) and step (2) adds in the extraction kettle together; Speed with 0.02-0.20 L/h in extraction kettle adds mass concentration 50-80% ethanol water entrainer; Or the adding mass concentration is a 50%-80% methanol aqueous solution entrainer; Or add the acetone entrainer or add the ethyl acetate entrainer, be to carry out supercritical CO extraction 0.5h-2.5 h under the 10-40 MPa at temperature 35-60 ℃ with pressure, in knockout drum, be 20-40 ℃ then with the temperature; Pressure is to isolate CO under the 4-7 MPa, obtains the solution of oil-containing tea polyphenols;

(5) step (4) gained oil-containing tea polyphenols solution decompression is steamed entrainer, obtain pale yellow powder shape solid.